Sputter Targets And Methods Of Forming Same By Rotary Axial Forging

ABSTRACT

A method of making sputter targets using rotary axial forging is described. Other thermomechanical working steps can be used prior to and/or after the forging step. Sputter targets are further described which can have unique grain size and/or crystal structures.

This application is a divisional of U.S. patent application Ser. No.11/121,440, filed May 4, 2005, which in turn claims the benefit under 35U.S.C. §119(e) of prior U.S. Provisional Patent Application No.60/568,592 filed May 6, 2004, which is incorporated in its entirety byreference herein.

BACKGROUND OF THE INVENTION

The present invention relates to sputter targets and components used forsputtering. More particularly, the present invention relates to methodsof forming sputtering targets as well as the sputtering targetsresulting from the methods of the present invention.

There are a variety of ways to make sputtering targets from metals whichgenerally involves taking a powder metallurgy product or a ingot-derivedproduct which is generally in the shape of a billet and subsequentlyworking the billet into the shape of the desired sputter target whichmany times is planar and circular. The means generally used to work abillet into the desired shape are various methods of forging which arerolling, hammer milling, extruding, upset forging, and the like.Generally, these methods are work intensive in that they take largeamounts of time to work the material since these forging or millingoperations are very labor intensive and take a great amount of time dueto the necessary deformation that is involved. Furthermore, by usingthese type of forging or milling steps, a sputter target which isformed, generally requires large amounts of machining in order to obtainthe desired close tolerances and good surface finish. In addition, thecircular shape of the planar target is generally not exact and has alarge variance, such as a variance of 10 to 15%, with respect to thevariation in diameter around the target.

Thus, there is a need in the industry to overcome these disadvantagesand provide a lower cost method to form sputter targets as well asprovide a means to reduce the time necessary to form targets.

SUMMARY OF THE PRESENT INVENTION

A feature of the present invention is to provide a method to producesputter targets at a lower cost and with less labor intensiveoperations.

A further feature of the present invention is to provide a method tomake sputter targets which require less time during the formationprocess.

An additional feature of the present invention is to provide a methodthat provides a more consistent sputter target with respect to grainsize and/or crystal orientation.

An additional feature of the present invention is to provide a sputtertarget that has less variation in diameter around the target.

In addition, another feature of the present invention is to provide asputter target which, after formation, requires reduced machining.

A further feature of the present invention is to provide a sputtertarget that has a transitional primary texture or a controlled texturegradient.

Additional features and advantages of the present invention will be setforth in part in the description that follows, and in part will beapparent from the description, or may be learned by practice of thepresent invention. The objectives and other advantages of the presentinvention will be realized and attained by means of the elements andcombinations particularly pointed out in the description and appendedclaims.

To achieve these and other advantages, and in accordance with thepurposes of the present invention, as embodied and broadly describedherein, the present invention relates to a method of forming a sputtertarget. The method involves rotary axial forging of an ingot derivedpreform to a shape and size of a sputter target. The rotary axialforging is preferably achieved in a closed die.

The present invention further relates to a sputter target having a grainsize pattern that is a continuous radial-circumferential pattern aroundthe center of the sputter target.

Furthermore, the present invention relates to a sputter target having acrystal structure pattern that is a continuous radial-circumferentialpattern around the center of the target.

Also, the present invention relates to a sputter target having avariation in diameter of no more than 5% around the sputter target.

In addition, the present invention relates to a sputter target having atransitional primary texture or controlled texture gradient.

It is to be understood that both the foregoing general description andthe following detailed description are exemplary and explanatory onlyand are intended to provide a further explanation of the presentinvention, as claimed.

The accompanying drawings, which are incorporated in and constitute apart of this application, illustrate several embodiments of the presentinvention and together with this description, serve to explain theprinciples of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS

FIGS. 1 (A)-(C) are side exploded views of the general working of abillet into a sputter target by rotary axial forging.

FIGS. 2 (A)-(C) is a side exploded view of the rotary axial forging of astarting billet using a bottom die.

FIG. 3 is a flow diagram of side views of the sequential process offorming a sputtering target using one embodiment of the presentinvention.

FIG. 4 is an EBSD cross-section showing the grain structure andorientation of a rotary axial forged tantalum sputtering targetmaterial.

FIG. 5 is an EBSD derived pole figure from a rotary axial forgedtantalum sputtering target material.

FIGS. 6-8 are graphs showing texture gradients for % (111), % (110), and% (100) respectively, through the thickness of the samples.

FIG. 9 is a graph showing the average grain size through the thicknessof the samples.

DETAILED DESCRIPTION OF THE PRESENT INVENTION

The present invention relates to sputter targets and methods of makingsputter targets preferably using a rotary axial forging technique aspart of the method of forming the sputter target.

In more detail, in the process, a sputter target can be formed by rotaryaxial forging of an ingot derived preform or work piece to the shape andsize of the desired sputter target.

For purposes of the present invention, the ingot derived preform workpiece can be any ingot derived material that can be reduced in size(e.g., deformation) to the shape of the desired sputter target. Thus,the ingot derived preform is a material that generally has a greaterheight than the desired sputtering target and a lesser diameter than thesputter target. The ingot derived preform can generally be any desiredheight and/or diameter or other dimensional shape as long as it can beshaped or deformed or worked to the desired shape of the final sputtertarget dimensions. For purposes of the present invention, preferably,the ingot derived preform is cylindrical in shape and can be, forinstance, a billet, a rod, a cylinder, or other similar shape. The ingotderived preform can have other geometrical shapes such as a rectangle.However, starting with this type of preform shape generally results intaking the rectangular shape and forming it into a cylindrical shape byforging techniques known to those skilled in the art. As an example, abillet having a diameter from about 3 inches to about 14 inches can beused. Generally, the height of the billet is preferably no more thanabout 2 times and more preferably no more than 1.8 times the diameter ofthe billet or other preform or other work piece. Larger height/diameterratios can be used.

The billet or other work piece can be formed, for instance, followingthe methods and techniques described in U.S. Pat. No. 6,348,113 toMichaluk et al., incorporated in its entirety by reference herein.

With respect to the ingot derived preform, the preform can have anypurity, any grain size, and/or any texture. Preferably, the ingotderived preform has a purity of greater than 95% with respect to theprimary metal present and more preferably a purity of 99%, 99.5%, 99.9%,99.95%, 99.99%, 99.995%, 99.999%, or greater with respect to the purityof the primary metal present. With respect to the metal, any metal canbe used as long as it can be sputtered. BCC-type or FCC-type metals oralloys thereof can be used. Examples include, but are not limited to,refractory metals, valve metals, as well as other types of metals.Specific examples include, but are not limited to, tantalum, niobium,titanium, cobalt, copper, aluminum, gold, silver, nickel, platinum,hafnium, zirconium, paladium, vanadium, iridium, molybdenum, tungsten,iron and alloys thereof, and the like.

As stated, the ingot derived preform can have any average grain size.Examples of average grain sizes include 1,000 microns or less and morepreferably 500 microns or less. Other ranges include, but are notlimited to, 250 microns or less, 150 microns or less, 100 microns orless, 75 microns or less, 50 microns or less, 25 microns or less, 10microns or less, and any other numerical ranges from about 1 micron toabout 1,000 microns. With respect to the texture, any crystalorientation can be used in the present invention. Examples include, butare not limited to, primary textures and mixed textures. For instance,the texture can be, for cubic metals, a (111) texture (or crystalorientation), a (100) texture, a (110) texture, or a mixture of thesetextures. Similarly, for hexagonal metals such as titanium, the texturecan be (0002) texture, (10 12) texture, (10 10) texture, or a mixture ofthese textures. The texture can be throughout the ingot derived preformand/or on the surface. Preferably, the texture is uniform, but it is notnecessary. Also, preferably, but not necessary, the cubic metal texturescan be without any textural banding. For instance, the ingot derivedpreform can be substantially void of (100) textural banding.

In the present invention, the ingot derived preform is subjected torotary axial forging. This rotary axial forging may also be known asorbital forging. Preferably, the rotary axial forging is done inassociation with a closed die. Any rotary axial forging machine can beused. Examples include, but are not limited to, rotary axial forgingmachines commercially available from VSI Automation, Auborn Hills, Mich.(VSI OFP-100), Wagner Banning, Dortmund, Germany (AGW-125 or AGW-400),Schmid Corporation, Switzerland (Model T630 or T200) In addition, rotaryaxial forging machines are further described in U.S. Pat. Nos.4,313,332; 4,795,333; and 5,531,088, which are all incorporated in theirentirety by reference herein. Also, various aspects of rotary or axialforging are further described in “Past Developments and Future Trends inthe Rotary or Orbital Forging Process,” Shivpuri, R., J. Mater. ShapingTechnol. 6, (1) 1988, PP. 55-71; “The Push Toward Orbital Forging,”Honegger, H. R., Am. Mach. 126, (11) November 1982, pp. 142-144; “OrbialForging of Heavy Metal EFP Liners,” Faccini, E. C., ConferenceProceedings; “High Strain Rate Behavior of Refractory Metals and Alloys,TMS, Warrendale, Pa., 111 (1992); “Metallurgical Aspectis of RotaryMetal Forming,” Standring, P. M.; Moon, J. R., “Rotary MetalworkingProcesses,” 1979, PP. 157-170, IFS (Conferences) Ltd and University ofNottingham, November 1979; “Recent development and applications ofthree-dimensional finite element modeling in bulk forming processes,” J.Mater. Process. Technol., Vol. 113 No. 1-3 2001/June PP. 40-45;“Load-Deformation Relationships during Upsetting by Rotary Froging”, R.E. Little and R. Beyer, “Rotary Metalworking Processes,” 1979, pp.157-170, IFS (Conferences) Ltd and University of Nottingham, November1979; “Deformation Characteristics of Cylindrical Billet in Upsetting bya Rotary Forging Machine”, K. Kubo and Y. Hirai, “Rotary MetalworkingProcesses,” 1979, pp. 157-170, IFS (Conferences) Ltd and University ofNottingham, November 1979; “Orbital Forging”, J. R. Maicki, Metallurgiaand Metal Forming, June, 1977, pp. 265-269, wherein all of thesereferences are also incorporated in their entirety by reference herein.

With respect to the operation of the rotary axial forging, the amount ofpressure or force applied by the rotary axial forging can be from about50 tons to about 700 tons (or more) and more preferably from about 200to 630 tons. Generally, the ingot derived preform is rotating at a speedof from about 30 rpm to about 120 rpm (or more) and more preferably fromabout 50 rpm to about 80 rpm during the orbital forging step. The rotaryaxial forging machine having an upper platen, which is the platen thatactually contacts the ingot derived preform while the forging operation,preferably, rotates at a speed of from 30 rpm to about 300 rpm and morepreferably from about 100 rpm to about 240 rpm during the orbitalforging. Generally, during the forging step, the temperature of theingot derived preform is at a temperature of from about −196 to about1000° C., and more preferably from about 20° C. to about 350° C.

The contact area of the die to the billet and the yield strength of thematerial to be forged are factors in determining the size of the rotaryforging machine required for manufacturing the sputtering target. Thecontact area in orbital forging can be calculated using the equation:A=πR²(0.48 h/(2 R tan(α))^(0.63) where A is the contact area, R is theradius of the billet, h is the depth of feed/revolution and α is thetilt angle between the upper die and the billet plane. The force (F)required from the rotary forging press to form a sputtering target ofradius R is given by the equation; F=A Y C, where Y is the flow stressof the metal billet material and C is the constraint factor. Theconstraint factor multiplied by the yield strength of the material canbe viewed as an effective yield strength for the rotary forging processthat takes into account the frictional forces in the die.

During the rotary axial forging step, the ingot derived preform can bereduced to the desired shape and size of the sputter target in a matterof seconds such as 1 minute or less and more preferably 30 seconds orless which, needless to say, results in a great reduction in theformation time of a target.

In the rotary axial forging step, preferably, a closed die is used whichis in the shape and size of the desired sputter target. Essentially,this die or mold permits the ingot derived preform to deform into theexact desired shape and size of the sputter target and results in a verylow variance in the finish product with respect to the variance indiameter of the sputter target. Generally, using the present invention,the variance in the diameter around the target is 5% or less.

In addition, with rotary forging it is possible to form the sputteringtarget so that its shape conforms to the erosion pattern of thesputtering target. This conserves material and reduces material cost forthe sputtering target.

The closed die can be made from any material such as tool steel, orsimilar material. Lubricants such as molybdenum disulfide or similar orother types of forging lubricant can be used to reduce friction forcesduring forging.

In the present invention, the ingot derived preform that is subjected torotary axial forging can be annealed or unannealed. Preferably, theingot derived preform is annealed. More preferably, for tantalum theingot derived preform is annealed at a temperature of from about 900° C.to about 1200° C. for a time of from about 60 minutes to about 240minutes, preferably in a vacuum or inert atmosphere. The ingot or metalarticle can be coated as well. Other temperatures and/or times can beused. Any number of anneals can be used.

The size of the ingot derived preform which is forged in the presentinvention is typically based on the desired finish size of the sputtertarget. In other words, once one knows the size of the sputter target,one can readily determine the volume of metal in that sputter target andthen decide on an appropriate diameter and height of the starting ingotderived preform, such that the starting ingot derived preform hasessentially the same volume as the finished sputter target. Preferably,the height of the ingot derived preform is no more than about 3 timesgreater than the diameter of the ingot derived preform. More preferably,the height is closer to 1.8 times or is 1.8 times the diameter of theingot derived preform. Generally, the height is not over 3 times, thoughit is possible, however it is not preferred.

The final shape or size of the sputter target can be any size such asconventional sizes like 6 inches to 18 inches with a height of fromabout 0.125 to about 1 inch.

As an option, prior to the rotary axial forging step, the ingot derivedpreform can be subjected to a first thermomechanical working ordeformation step. In the present invention, it is preferred that theingot derived preform is subjected to this prior thermomechanicalworking, which can be in the form of any working means (preferably,other than orbital forging), such as rotary forging, hammer forging,upset forging, rolling, cross rolling, extrusion, and the like.Essentially any means to thermomechanically work the material can beused as long as the ingot derived preform is returned to a cylindricalshape for purposes of rotary axial forging. Thus, the ingot derivedpreform could, in one embodiment, be rolled to any geometrical shape aslong as it is subsequently return to a cylindrical shape for purposes ofthe preferred embodiment of the present invention. The priorthermomechanical working or deformation of the ingot derived preformpreferably provides improved grain size and/or improved texture in thepreform. Furthermore, the prior thermomechanical working can be done toobtain a preform that has the necessary size and/or shape for purposesof being subjected to a particular rotary axial forging machine. Forinstance, a billet having a diameter, for instance, in the range ofapproximately 3 inches to approximately 14 inches can be subjected to afirst thermomechanical working, such as forging, to reduce the diameterby at least 5% and more preferably at least 50% and even more preferablyat least 100% of the original starting diameter. This deformation andreduction in size can be even greater than 100% if desired. The workingof the preform can be cold or hot working or combinations thereof. Thebillet can be worked again to restore the original diameter.

For purposes of the present invention, there can be more than one priorthermomechanical working prior to the rotary axial forging step. Anynumber of working steps prior to the rotary axial forging can be done inorder to achieve any desired percent deformation or otherthermomechanical working of the preform.

In another embodiment of the present invention, the rotary axial forgingcan occur in stages. For instance, if the rotary axial forging devicedoes not have enough tonnage to forge the overall free form, radialdisplacement can be provided on the lower die so that the orbitalforging can be done in multiple steps. For instance, the inner portionof the plate can be formed by orbital forging up to the tonnage limit ofthe machine, wherein the inner portion has a radius that is less thanthe final radius of the part. Thus, if one wanted to form a 13 inchdiameter plate, the first 8 inches of the plate can be formed with theupper and lower dies aligned on center. Then, the outer portion of thepreform can be forged in the same manner by moving the upper platen tothe parts of the preform which have not previously been forged. In thealternative, or in combination, the lower platen which the preform restsupon can be moved such that it is aligned with the upper platen forforging the previously unforged area. Thus, by this method, an overalllarge preform which previously could not be forged in one orbitalforging step can be forged by orbital forging in two or more steps whichpreferably occur sequentially. Thus, the die or upper platen is simplymoved or the lower platen is moved in order to uniformly forge theentire preform in order to achieve the desired shape and final thicknessof the material, such as in the form of a sputter target. For example,to form a 13 inch diameter plate, one can first forge the first 8 inchesof the plate with the upper and lower dies aligned on center. The outerportion of the billet or preform would then be unformed with the innereight inch diameter formed to near final thickness. Then, the lower diecan be translated by the radius of the first pressing, in this example,the translation rate is 4 inches. Then, the second orbital forgingpressing can occur to form the outer diameter portion. This pressingforms that outer portion to the final 13 inch diameter. This two stepmethod reduces the maximum force required for orbital forging. Thismultiple step process can be repeated any number of times to form evenlarger diameter plates while only using the force available from theorbital forging press that is being used. Numerous advantages areprovided by this multi-step method. In the alternative, one can pressradially inward starting at the outer diameter portion and move inwardsor one can first press radially starting at the inner diameter and moveoutwards in one or more steps.

After the rotary axial forging step, any number of other conventionalsteps can be preformed on the sputter target. For instance, the sputtertarget can then be annealed any number of times using similar annealingparameters as described above for the optional annealing step.

Also, the sputter target can optionally be subjected to any furtherthermomechanical working steps, such as a rolling step, flattening step,or other thermomechanical working such as drawing, hydroforming,superplastic forming, spinning or flow forming or any combination ofthermomechanical workings.

Also, the sputter target can optionally be subjected to machining,grinding, lapping, milling or polishing in order to obtain desiredspecifications.

Once the desired sputter target is obtained, the sputter target can thenbe affixed to a backing layer or plate to complete the target assembly.The affixing of the sputter target to the backing plate can be done byany attachment means such as diffusion bonding, friction brazing,friction welding, explosion bonding, soldering, and the like. As anoption, at least one interlayer can be located between the sputtertarget and backing layer and the interlayer can be affixed to the targetor to the backing plate or both prior to affixing the target assemblytogether. The backing plate can be any conventional material such ascopper, aluminum, titanium, or alloys thereof.

As indicated, at least one surface of the sputter target can be machinedto desired properties and tolerances.

With respect to the sputter target obtained in the present invention, inone embodiment, the sputter target preferably has a grain size patternthat is a continuous radial-circumferential pattern which is around thecenter of the target. Thus, the grain size pattern is unique withrespect to the fact that it is circular around the center of the targetbut also radiates out to the outer diameter of the target. Essentially,the grain size pattern is a blending of a radial pattern with acircumferential pattern. The sputter target, in one embodiment of thepresent invention, with this unique blending of grain size pattern,provides unique properties with respect to uniform sputtering especiallysince the circular pattern can better match the circular pattern of themagnets in sputtering equipment. Thus, the sputter target not onlyprovides a more uniform thin film on a substrate but also the sputtertarget sputters or erodes uniformly which provides a more efficient andcomplete use of the sputter target. Similarly, the sputter target, inthe same embodiment or a separate embodiment can have a crystalstructure pattern that is a continuous radial-circumferential pattern.This crystal structure, as indicated above, can have any texture. Again,this preferred continuous radial-circumferential pattern in textureprovides a more uniform target which leads to, in preferred embodiments,uniform erosion as well as the formation of a uniform thin film on thedesired substrate.

For purposes of the present invention, the sputter target resulting fromthe methods of the present invention can have the same or differenttexture and/or grain size as the starting ingot derived preform. Thus,with respect to the grain sizes and texture and purities specified abovewith respect to the preform, these parameters can equally be present inthe finished sputter target.

In one embodiment of the present invention, the sputter target hasdesirable metallographic structure. For instance, the crystallographictexture of the target can be a transitional primary texture through thethickness of the target. For example, one end of the target (forinstance, the top side portion of the target) can have a primary textureof (110) and the other end of the target (e.g., the lower side portionof the target) can have a primary texture of (111). This shifting ofprimary textures through the thickness of the target can be verybeneficial for sputtering purposes. Another way of describing thebeneficial attributes of this embodiment is that the target has texturegradients through the thickness of the target wherein a stronger textureis present at certain locations of the target. The transitional primarytexture or texture gradient is very beneficial in sputtering in order tocompensate for a variation in sputter rate as the target erodes. Theprocess of the present invention produces a unique texture that has notbeen observed in other metal working processes. In at least oneembodiment of the present invention, the present invention produces anear linear texture gradient through the thickness of the target ormetal article which can be used to compensate for natural variations insputter rate that occurs with creation of a sputter erosion track in thesputtering target. The sputtering rate in a target tends to decreasewith sputtering time at constant power because as the target sputters,the surface area of the target increases. This increased sputter arearesults in a reduced effect of applied power per unit area, which causesa reduction in the effective sputter rate. This effect is usuallycompensated for by gradually increasing the power applied to thesputtering target as it erodes. In the present invention, by introducinga controlled texture gradient or transitional primary texture in thesputtering target, the sputtering target can be shifted from a highsputtering rate texture, such as a (111) to a higher sputtering rateorientation, such as a (110) to compensate for the lower effective powerdensity. Examples of this texture gradient are further shown in theexamples, including FIGS. 6-8.

For purposes of the present invention, the transitional primary texturecan be any shifting of primary texture. For instance, and with referenceto the overall thickness of the target, one part of the sputter target,such as the upper part or lower part, more particularly, for instance,the upper half or lower half of the target can be a primary texture(e.g., a texture that is over 50% of overall texture or the highest % oftexture present amongst all textures) such as (111), (100), (110), or amixture of two or more of these textures. The other portion of thetarget or metal article is a different primary texture. Thus, as anexample, one portion of the target can have a primary (111) texture andthe other portion of the target can have a primary (100) texture. Inanother embodiment, one portion of the target can have a primary (111)texture and the other portion of the target can have a primary (110)texture. In another embodiment of the present invention, one portion ofthe target can have a primary (100) texture and the other portion of thetarget can have a primary (110) texture. In a further embodiment of thepresent invention, one part of the target can have a primary (100)texture and the other part of the target can have a primary (111)texture. Essentially, any combination of shifting primary textures canbe achieved. The “portion” or “part” containing the respective primarytexture can be from 10% to 90% of the overall top/bottom thickness ofthe target or metal article and more preferably is from 25% to 75% orfrom 35% to 60% of the overall thickness. For instance, in a 14 mm thicktarget, the first 5-6 mm of thickness, starting at the top, can be aprimary (111) which is about 40% of thickness, and remaining thicknesscan be a primary (110). Furthermore, in another embodiment of thepresent invention, the texture can shift from a primary texture to amixed texture. For instance, one portion of the target can have aprimary (111) texture and the other portion can have a mixed (111):(100)texture or a mixed (110):(100) texture, and the like. Preferably, thetexture that is initially exposed to sputtering is a texture which has alower sputtering rate texture than the portion of the target that issputtered afterwards which preferably has a higher sputtering rate. Asfurther examples, the texture gradient of the target or metal articlecan have a (111) plane or (111) texture ranging from −1%/mm to −10%/mmor more. Other examples of suitable texture gradients can include forthe (111) plane or (111) texture of from −2.5%/mm to −5.0/mm. Thisnegative texture gradient means that the minus sign indicates that the(111) texture is more predominant or primary in the upper thicknesses ofthe target and that the predominates of the (111) texture diminishes ina linear or near linear type fashion as the texture is measured throughthe depth in millimeters of the target. Thus, a −2.0%/mm would mean thatthe (111) texture will decrease on average, about 2% per millimeter ofthickness of target and thus, if the target is 14 millimeters thick, the(111) texture decreases about 24% from the top of the surface to thevery bottom of the surface of the same target. Similarly, a texturegradient can exist in the same target for a (110) texture wherein thetexture gradient starting from the same upper surface is 1%/mm to10%/mm, meaning that the texture will initially be lower in the uppersurface of the target and will gradually increase in a linear or nearlinear fashion throughout the target until the bottom of the target isreached. Other texture gradients for the (110) can include from about1%/mm to about 7%/mm or from about 1%/mm to about 5%/mm, or from about1% to about 4%/mm through the thickness of the target or metal article.Similar gradients can exist for the (100) texture. For othercrystallographic orientation, such as in FCC metals, a similar shiftingof orientations for various textures can be achieved. The presentinvention relates to at least one texture that exists in a target ormetal article that has a texture gradient which can be in a linear ornear linear fashion wherein near linear generally means that the texturewill generally increase or generally decrease throughout the thicknessof the target in a consistent manner within error such as within 10% orwithin 25% of the linear relationship.

The various texture gradients described above with respect to (111) canequally apply to (100) or (110). Similarly, the texture gradientprovided for (111) described above can equally apply to (110) or (100).In one embodiment, which can apply to the texture gradients given byexample above with respect to (111) and (100), the (100) texturegradient can be about 0%/mm to about 5%/mm, and other ranges includefrom about 0.5%/mm to about 3%/mm, or from about 0.5%/mm to about 2%/mmthrough the thickness of the target. The lower the texture gradientgenerally means that the texture is staying substantially the samethroughout the thickness. In one embodiment of the present invention,the (100) texture gradient is low, such as below 3%/mm which reflectsthat the (100) texture is generally about the same throughout thethickness of the target. Again, this low texture gradient can equallyapply to (111) or (110) depending on the type of texture gradientsdesired in the targets. In one preferred embodiment of the presentinvention, the texture gradient for the (111) texture is a negativetexture gradient and the (110) texture gradient is a positive texturegradient and the (100) texture gradient is a near 0 texture gradientsuch as 3%/mm or less. In another embodiment of the present invention,the target or metal article can have at least one positive texturegradient for one or more textures and/or at least one negative texturefor one or more textures, and/or a 0 or near 0 texture gradient for oneor more textures. Any of the various combination of texture gradients ortransitional primary textures can exist along with a grain sizevariation through the thickness which is very low such as an averagegrain size throughout the thickness of the target that does not varybeyond +/−50 microns and more preferably does not vary +/−25 micronsthroughout the thickness of the target. In other words, if the averagegrain size as measured at 2 mm depth is about 25 microns, the averagegrain size throughout the depth of the target will not exceed 75 micronsand will preferably not exceed 50 microns in average grain size. Thisconsistent average grain size range throughout the thickness of thetarget is also beneficial from a uniform sputter rate and film thicknessformation point of view. One example of the small grain size variationis shown in FIG. 9 in the examples.

Furthermore, in one embodiment, the sputter target preferably has avariation in diameter of 5% or less (e.g., 4%, 3%, 2%, or 1% or less).This control in variance is highly desirable with respect to uniformsputtering and complete erosion of the sputter target.

With respect to the Figures, FIG. 1 sets forth an example of the processof the present invention wherein a starting billet, shown in FIG. 1A, issubjected to a rotary axial forging. The top die is applied to thestarting billet as an axial force to cause the flow of the metalmaterial in order to form the desired diameter of the sputter target, asshown in FIGS. 1B and 1C. FIG. 2A shows in this embodiment a startingbillet which is subjected to a top die form having a different type ofdesign. Axial forces are applied to the starting billet to cause thematerial flow of the metal. The starting billet or work piece is atleast partially located in a bottom die in order to control the finalconfiguration of the finished target which is shown in FIG. 2C. FIG. 3shows a flow diagram of one embodiment wherein a starting billet issubjected to a prior forging step to reduce the diameter and thensubjected to a second forging step to increase the diameter. Then, thework piece or preform is subjected to a rotary axial forging step toincrease the diameter to 18.5 inches. Afterwards, this piece which isessentially in the shape of the desired sputter target is then subjectedto a vacuum anneal and can be attached to a backing plate and thensubjected to final processing steps including final machining. FIG. 4shows the Electron Backscattered Diffraction map of the cross-section ofan orbitally forged tantalum plate after annealing at 1050 C. In thispresentation grains with (111) planes parallel to the target plane arecolored blue (darkest colored regions in Figure), grains with (110)planes parallel to the target plane are colored green (lightest coloredregions in Figure) and grains with their (100) planes parallel to thetarget plane are colored red (essentially only present in {111} Polefigure as two spots). The texture gradient through the target is easilyseen. FIG. 5 provides the EBSD pole figure for this material.

The present invention will be further clarified by the followingexamples, which are intended to be exemplary of the present invention.

Example

Table 1 summarizes the experimental conditions used for rotary forginghigh purity tantalum for use in the manufacture of sputtering targets.The experimental conditions were used to produce tantalum plates ofapproximately 11 inches in diameter. For commercial sputtering targets,tantalum blanks with 13 to 18 inches in diameter are useful. Thecalculations of the force required for these larger diameter plates isprovided at the bottom of Table 1. In Table 1, Sample 1A, 1B, 2A, and 2Bwere annealed prior to orbital forging for 1050 deg C. in vacuum for 2hours soak. Samples 1A and 1B were extruded prior to annealing, goingfrom a 11 inch ingot to a 3.54 inch billet and 5.9 inches long. Samples3A and 3B were also extruded as in 1A, but with no annealing. Samples 2Aand 2B were rotary forged going from a 11 inch ingot to a 3.54 inchbillet and 5.9 inches long and annealed as discussed after rotaryforging. Samples 4A and 4B were also rotary forged but no annealing.

TABLE 1 Orbital Forging Experimental Conditions Rotary Forge: AWG-160Tantalum Yield 30 Strength (kpsi) Die Angle (deg) 10 Billet Diameter(in) 3.6 Rotation Rate (rpm) 240 Billet Height (in) 6 Plate radius after5.43 forging (in) Sample No. 1A 1B 2A 2B 3A 3B 4A 4B Feed/Rotation 0.1080.108 0.054 0.163 0.163 0.054 0.108 0.244 (in/rev) Applied Force (ton)144 144 155 155 159 164 184 187 Billet Temp (C.) 297 335 305 305 339 290300 320 Upper Die Temp (C.) — 150 150 150 140 120 130 130 Lower Die Temp(C.) — 90 100 89 100 100 113 120 Calculated Contact 3.2 3.2 1.6 4.9 4.91.6 3.2 7.3 Area (in2) Effective Yield 89 89 191 63 65 202 114 51Strength (kpsi) 13 in Dia Contact 4.2 4.2 2.1 6.3 6.3 2.1 4.2 9.4 Area(in2) 13 in Dia Force 185 185 199 199 205 211 237 241 (tons) 18 in DiaContact 6.6 6.6 3.3 9.9 9.9 3.3 6.6 14.9 Area (in2) 18 in Dia Force 292292 314 314 323 333 373 379 (tons)

One of the tantalum sputtering targets fabricated by rotary closed dieforging was analyzed for metallographic structure. This material,designated as sample 2B in Table 1, had an average grain size of 36 μmand was uniform within 10 μm from the top to bottom of the 0.5 inchthick plate. The crystallographic texture of this plate averaged around45% (111), 20% (110) and 35% (100). The (111) crystallographic texturenear the plate bottom was near 80% and decreased to near 20% near thetop surface of the plate. This texture gradient can be used to takeadvantage in the design of sputtering targets by using the texturegradient to compensate for the normal reduction in sputtering rate thatoccurs with the continued erosion of the sputtering target. By placingthe higher sputtering rate texture in the target toward the back surfaceof the target, the normal reduction in sputtering rate can be reduced.

FIG. 6 provides the crystallographic texture gradient found in orbitalforged tantalum plate. Texture gradients for the (111) planes range from−3.8%/mm to −4.9%/mm in this data set. The high % (111) in the left sideof the graph occurs on the tantalum sample side that is adjacent to thelower die where the tantalum billet and the die are not moving relativeto each other. The low % (111) on the right side of the graphcorresponds to the sample face that is in contact with the rotating dieand is experiencing high shear.

FIG. 7 provides a similar series of curves for the % (110)crystallographic texture. In this case, the % (110) texture graduallyincreases as one goes from the left to right side corresponding tomoving from the stationary lower die contact surface to the upperrotating die contact surface in the tantalum plate. In this case thetexture gradients range from 1%/mm to 4.1%/mm as one moves from thestationary die contact surface to the rotating die contact surface.

FIG. 8 provides the through thickness texture variation for the % (100)texture component for orbital forged tantalum plate. The % (100) texturegradient ranged from 3%/mm to 0.7%/mm. The gradient in the (100)component tends to be less than the gradients in the (111) and (100)component.

The grain size variation through thickness in orbital forged tantalumplate is provided in FIG. 9. The grain size shows only a slight gradientthrough thickness in the orbital forged tantalum. Average grain sizeranges from 25 to 50 μm with the grain size slightly larger in thematerial near the lower die that is stationary relative to the tantalumbillet.

Table 2 provides a summary of the measured texture gradients and grainsize for the four tantalum samples described in this application.

TABLE 2 % (111) % (100) % (110) Slope Slope Slope (%/ Intercept (%/Intercept (%/ Intercept Avg GS Trial mm) (%) mm) (%) mm) (%) (um) 1 −3.885 2.1 17 1.7 −2 27 2 −4 75 3 18 1 6 28.9 3 −4.8 72 0.7 33 4.1 −4 48.6 4−4.9 72 2.2 23 2.6 5 38.1

Applicants specifically incorporate the entire contents of all citedreferences in this disclosure. Further, when an amount, concentration,or other value or parameter is given as either a range, preferred range,or a list of upper preferable values and lower preferable values, thisis to be understood as specifically disclosing all ranges formed fromany pair of any upper range limit or preferred value and any lower rangelimit or preferred value, regardless of whether ranges are separatelydisclosed. Where a range of numerical values is recited herein, unlessotherwise stated, the range is intended to include the endpointsthereof, and all integers and fractions within the range. It is notintended that the scope of the invention be limited to the specificvalues recited when defining a range.

Other embodiments of the present invention will be apparent to thoseskilled in the art from consideration of the present specification andpractice of the present invention disclosed herein. It is intended thatthe present specification and examples be considered as exemplary onlywith a true scope and spirit of the invention being indicated by thefollowing claims and equivalents thereof.

1. A method of forming a sputter target comprising rotary axial forgingof an ingot derived preform to the shape and size of said sputtertarget.
 2. The method of claim 1, wherein said ingot derived preform isa valve metal or refractory metal.
 3. The method of claim 1, whereinsaid ingot derived preform is a tantalum preform or alloy thereof. 4.The method of claim 1, wherein said ingot derived preform is a titaniumpreform or alloy thereof.
 5. The method of claim 1, wherein said ingotderived preform is a niobium preform or alloy thereof.
 6. The method ofclaim 1, wherein said ingot derived preform is a cobalt, copper,aluminum, gold, or silver preform, or alloys thereof.
 7. The method ofclaim 1, wherein said ingot derived preform comprises tantalum, niobium,titanium, combinations thereof, or alloys thereof.
 8. The method ofclaim 1, further comprising thermomechanically working said ingotderived preform prior to said rotary axial forging.
 9. The method ofclaim 1, further comprising reducing the diameter of said ingot derivedpreform by working of said preform prior to said rotary axial forging.10. The method of claim 9, wherein said reducing in diameter is achievedby forging, rolling, or combinations thereof.
 11. The method of claim 1,wherein said ingot derived preform is annealed prior to said rotaryaxial forging.
 12. The method of claim 1, further comprising annealingsaid ingot derived preform at a temperature of from about 900° C. toabout 1200° C. for a time of from about 60 minutes to about 240 minutesprior to said rotary axial forging step.
 13. The method of claim 1,wherein said rotary axial forging is achieved by rotating the ingotderived preform at a speed of from about 30 rpms to about 300 rpms andwherein said rotary axial forging has an upper platen which rotates at aspeed of 30 rpms to about 300 rpms during said rotary axial forgingstep.
 14. The method of claim 1, wherein said ingot derived preform is abillet, rod, or cylinder.
 15. The method of claim 1, wherein said shapeand size of said sputter target is not the finished shape and size of asputter target and wherein said method further comprises subjecting saidsputter target to further thermomechanical working in order to obtainthe desired shape and size of a finished sputter target.
 16. The methodof claim 1, wherein said method further comprises machining at least onesurface of said sputter target.
 17. The method of claim 1, furthercomprising affixing said sputter target to a backing plate.
 18. Themethod of claim 1, further comprising affixing at least one interlayerto said sputter target or to said backing plate, or both and thenaffixing said target, plate, and interlayer together to form a targetassembly.
 19. The method of claim 1, further comprising rolling,flattening, milling, grinding, lapping, polishing, or combinationsthereof to said ingot derived preform or to said sputter target or toboth.
 20. The method of claim 1, wherein said ingot derived preform iscylindrical in shape and has a height that is no more than 3 times thediameter.
 21. The method of claim 9, wherein said ingot derived preformis reduced in diameter by at least 5%.
 22. The method of claim 1,wherein said ingot derived preform is reduced in diameter by at least10%. 23-28. (canceled)
 29. The method of claim 1, wherein said rotaryaxial forging occurs in a closed die.
 30. The method of claim 29,wherein said closed die is in the shape of the sputter target.
 31. Themethod of claim 1, wherein said sputter target has an average grain sizeof from about 20 to about 100 μm.
 32. The method of claim 31, whereinthe sputter target comprises aluminum, copper, tantalum, niobium,titanium, platinum, gold, nickel, iron, vanadium, molybdenum, tungsten,silver, palladium, iridium, zirconium, hafnium or alloys thereof, orcombinations thereof.
 33. The method of claim 31, wherein said sputtertarget is tantalum with purity of at least 99.99%.
 34. The method ofclaim 31, wherein said sputter target is tantalum with an averagecrystallographic texture that is primary (111).
 35. The method of claim31, wherein said sputter target is tantalum with an averagecrystallographic texture that is primary (110).
 36. The method of claim1, wherein said rotary axial forging occurs in two or more forging stepsof the ingot derived preform. 37-53. (canceled)